SYNTHESIS AND NUCLEAR-MAGNETIC-RESONANCE STUDIES OF SOME ETHYLENE AND ETHYLTRIS(PYRAZOLYL)BORATOIRIDIUM COMPLEXES

被引：27

作者：

CIRIANO, MA ^{[1
]}

FERNANDEZ, MJ ^{[1
]}

MODREGO, J ^{[1
]}

RODRIGUEZ, MJ ^{[1
]}

ORO, LA ^{[1
]}

机构：

[1] UNIV ZARAGOZA,CSIC,INST CIENCIA MAT ARAGON,DEPT QUIM INORGAN,E-50009 ZARAGOZA,SPAIN

来源：

JOURNAL OF ORGANOMETALLIC CHEMISTRY | 1993年 / 443卷 / 02期

关键词：

D O I：

10.1016/0022-328X(93)80304-T

中图分类号：

O61 [无机化学];

学科分类号：

070301 ; 081704 ;

摘要：

The synthesis of [Ir{HB(pz)3}(C2H4)(CO)] (2), [Ir{HB(pz)3}(C2H5)(eta2-C2H4)][BF4](3), and [Ir{HB(pz)3}(C2H5)(CO)][BF4](4) is described. Compound 2 is prepared by reaction of [Ir{HB(pz)3}(C2H4)2] (1) with carbon monoxide followed by treatment with ethylene under atmospheric pressure. Treatment of 1 and 2 with HBF4 affords compounds 3 and 4, respectively. Complex 2 is fluxional and its frozen structure is trigonal bipyramidal with the ethylene in the equatorial plane and the carbonyl group in one axial position; no rotation of the olefin is detected. Complexes 3 and 4 are square-pyramidal and are rigid on the nuclear magnetic resonance (NMR) time scale. These structural inferences are based on H-1 and C-13 NMR spectra for the complexes and nuclear Overhauser effect (NOE) measurements for 2.

引用

页码：249 / 252

页数：4

共 24 条

[1] PHOTOCHEMICAL-REACTIONS OF TRICARBONYL[HYDROTRIS(1-PYRAZOLYL)BORATO]RHENIUM(I) IN THE PRESENCE OF NEUTRAL DONOR LIGANDS - X-RAY CRYSTAL-STRUCTURES OF THE SUBSTITUTION DERIVATIVES [RE(HB(PZ)3)(CO)2L], WITH L = C4H8O OR PPH3 [J].

ANGARONI, M ;

ARDIZZOIA, GA ;

DALFONSO, G ;

LAMONICA, G ;

MASCIOCCHI, N ;

MORET, M .

JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1990, (06) :1895-1900

[2] STEREOCHEMICALLY NON-RIGID BIS(OLEFIN)RHODIUM POLY(1-PYRAZOLYL)BORATO COMPLEXES .2. X-RAY CRYSTALLOGRAPHIC STUDIES - THE CRYSTAL AND MOLECULAR-STRUCTURES OF THE NORBORNADIENE, CYCLOOCTA-1,5-DIENE, AND DUROQUINONE COMPLEXES [J].

COCIVERA, M ;

FERGUSON, G ;

KAITNER, B ;

LALOR, FJ ;

OSULLIVAN, DJ ;

PARVEZ, M ;

RUHL, B .

ORGANOMETALLICS, 1982, 1 (09) :1132-1139

[3] STEREOCHEMICALLY NON-RIGID BIS(OLEFIN)RHODIUM POLY(1-PYRAZOLYL)BORATO COMPLEXES .3. H-1 AND RH-103 NUCLEAR MAGNETIC-RESONANCE STUDIES [J].

COCIVERA, M ;

FERGUSON, G ;

LALOR, FJ ;

SZCZECINSKI, P .

ORGANOMETALLICS, 1982, 1 (09) :1139-1142

[4] BOND CHARACTER AND CONFORMATIONAL EQUILIBRATION OF ETHYLENE- AND TETRAFLUOROETHYLENERHODIUM COMPLEXES FROM NUCLEAR MAGNETIC RESONANCE SPECTRA [J].

CRAMER, R ;

KLINE, JB ;

ROBERTS, JD .

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1969, 91 (10) :2519-+

[5] ACTIVATION OF A VINYL CARBON HYDROGEN-BOND IN A TRIS(PYRAZOLYL)BORATOIRIDIUM COMPLEX - THE X-RAY CRYSTAL-STRUCTURE OF [IRH(HB(PZ)3)(OMICRON-C8H13)(ETA-2-C8H14)] [J].

FERNANDEZ, MJ ;

RODRIGUEZ, MJ ;

ORO, LA ;

LAHOZ, FJ .

JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1989, (10) :2073-2076

[6]

FERNANDEZ MJ, 1991, POLYHEDRON, V14, P1595

[7]

FREEMAN RA, 1988, HDB NUCLEAR MAGNETIC, P198

[8] A RHODIUM COMPLEX THAT COMBINES BENZENE ACTIVATION WITH ETHYLENE INSERTION - SUBSEQUENT CARBONYLATION AND KETONE FORMATION [J].

GHOSH, CK ;

GRAHAM, WAG .

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1989, 111 (01) :375-376

[9] THEORY OF POLYHEDRAL MOLECULES .3. POPULATION ANALYSES AND REACTIVITIES FOR CARBORANES [J].

HOFFMANN, R ;

LIPSCOMB, WN .

JOURNAL OF CHEMICAL PHYSICS, 1962, 36 (12) :3489-&

[10] THEORY OF POLYHEDRAL MOLECULES .1. PHYSICAL FACTORIZATIONS OF SECULAR EQUATION [J].

HOFFMANN, R ;

LIPSCOMB, WN .

JOURNAL OF CHEMICAL PHYSICS, 1962, 36 (08) :2179-&

← 1 2 3 →